CN105367681A - Edible and medicinal fungal polysaccharide low-temperature normal-pressure plasma extraction method - Google Patents
Edible and medicinal fungal polysaccharide low-temperature normal-pressure plasma extraction method Download PDFInfo
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Abstract
An edible and medicinal fungal polysaccharide low-temperature normal-pressure plasma extraction method includes the first step of adsorption resin preprocessing, the second step of fungal polysaccharide primary extraction, the third step of low-temperature normal-pressure plasma extraction, the fourth step of porous adsorption resin extraction, the fifth step of alcohol precipitation and the sixth step of drying. The fungal polysaccharide prepared through extraction is prepared from lentinula edodes, hericium erinaceus, ganoderma lucidum, black fungi, grifola frondosa, white fungi, flammulina velutipes and any one or combination of edible and medicinal fungi containing polysaccharide compounds. According to the edible and medicinal fungal polysaccharide low-temperature normal-pressure plasma extraction method, the extraction period is shortened, the use amount of solvents is small, production efficiency is high, energy is saved, consumption is reduced, and extraction purity is high.
Description
Technical field
the present invention relates to the extracting method of effective constituent in a kind of pharmaceutical fungi and edible fungi, particularly a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method.
Background technology
edible and medicinal fungi polysaccharide refers generally to high molecular polymer that is isolated, that be made up of more than 10 monosaccharide units from the sporophore of edible and medicinal fungi, mycelium, fermented liquid.In the world, edible and medicinal fungi glycocalix is called " biological response modifier " (BiologicalResponseModifier is called for short BRM).Modern pharmacology research shows, it is that a class has the various biological function such as anti-infective, radioprotective, anticoagulation, hypoglycemic, prevention and therapy tumour, antifatigue, is important Natural Active Principles and protective foods.In recent years along with biological chemistry, biotechnology, biopolymer study the continuous appearance of these new technologies, novel method, make to develop rapidly the research of edible and medicinal fungi polysaccharide both at home and abroad.Report from the research of recent domestic about medicinal fungi polysaccharide, current focus mainly concentrates on: the nutrition of medicinal fungi and physiologically active are studied; The structural analysis of medicinal fungi polysaccharide; The cultivation technique of medicinal fungi; The extraction, purifying process research etc. of medicinal fungi polysaccharide.Although people have carried out comparatively extensive research to the aspect such as structure, biological activity, pharmacological function of fungus polysaccharide, how each fungus polysaccharide of high efficiency extraction has been badly in need of research further.
at present, the method such as the preparation method of native fungal polyose medicament mainly contains hot water, acid, alkali lixiviate are got.All can there is the continuous volatilization of organic solvent in these methods, cause energy dissipation, fund waste and environmental pollution in process of production.Recent year also has report to adopt ion exchange chromatography separation purification of epiphyte polysaccharide, the wide aperture ion exchange resin that the many employings of column chromatography medium are domestic, being characterized in that dynamic separation is effective, serialization degree is high, the cycle of operation is short, the renewable recycling of resin, equipment is simple, is an economic effective means.
it is 200910010855.1 that State Intellectual Property Office discloses an application number in 2009.8.26, name is called the patent of invention of " interface modification method of continuous P BO fiber reinforcement bimaleimide resin base composite material ", which disclose a kind of interface modification method of continuous P BO fiber reinforcement thermosetting BMI resin, smooth for solving current fiber-reinforced resin matrix compound material body structure surface, active group is few, design with technical problems such as the bad adhesion of resin matrix, its solution: pbo fiber is in plasma processing apparatus, lower temperature plasma technology is adopted to carry out surface modification to fiber, modified fiber and the cohesiveness of resin matrix are greatly improved, interface performance improves greatly, matrix material interlayer shearing resistance strengthens further, excellent in mechanical performance.
Summary of the invention
the object of this invention is to provide a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method, extracting cycle shortens, and solvent load is few, and production efficiency is high, and energy-saving and cost-reducing, DNA purity is higher.
object of the present invention is achieved through the following technical solutions:
a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method, comprises following processing step:
a, polymeric adsorbent pre-treatment:
after being soaked with deionized water by the S5428 resin anion(R.A) of 1.6cm × 100cm, dress post, uses deionized water balance resin, until the liquid flowed out is not muddy;
b, fungus polysaccharide tentatively extract:
(1) raw material pulverizing mixes with extraction agent
clean extracting the raw material preparing fungus polysaccharide, after cryodrying, be ground into the particle of 70 ~ 6000um, by its with extraction agent in mass ratio 1:3 ~ 1:10 mix;
(2) extract
above-mentioned raw materials and extraction agent mixed solution are carried out circumfluence distillation, Extracting temperature 45 ~ 100 DEG C, pH=5 ~ 8 in multifunctional multistage solvent circulation Dynamic Thermal refluxing extraction device, and under the condition of solvent refluxing rate 10 ~ 25%, refluxing extraction 50 ~ 100 minutes, obtains extracting solution;
(3) filter with concentrated
after the extracting solution of said extracted certain hour being passed through secondary wire gauzee filter or centrifuging, direct vacuum handling is in external circulation heating formula economic benefits and social benefits vacuum concentrator, at vacuum tightness 0.02-0.09MPa, concentrate 2 ~ 4 hours under temperature 40 ~ 90 DEG C of conditions, make the density of concentrated solution reach 1.1 ~ 1.40g/cm3;
(4) alcohol precipitation
above-mentioned concentrated solution is pumped into Alcohol-settling tank, and add by volume after 3 ~ 5 times of 97% alcohol stirs and leave standstill 50 ~ 150 minutes, obtain alcohol precipitation extract, alcohol used is more than food grade;
c, low-temperature atmosphere-pressure plasma extract:
the alcohol precipitation extract that step B (4) obtains is put into low-temperature atmosphere-pressure plasma treatment appts, processes with following processing parameter, obtain edible and medicinal fungi polysaccharide crude: discharge frequency is 5 ~ 30KHz; Extraction time is 5 ~ 13s; Discharge gas is ammonia, and flow velocity is 0.5 ~ 5ml/min;
d, macroporous adsorbent resin extract
the edible and medicinal fungi polysaccharide crude obtained by step C adds water, macroporous adsorptive resins in wet method in steps A, successively with concentration be 0.5,1.0,2.0, the NaCl solution of 3.0mol/L and 4.0mol/L carries out wash-out, the speed of wash-out is 2.0 ~ 10.0ml/min; By elutriant concentrating under reduced pressure, obtain edible and medicinal fungi polysaccharide macroporous adsorbent resin extract;
e, alcohol precipitation
the fungus polysaccharide macroporous adsorbent resin extract obtained by step D pumps into Alcohol-settling tank, adds by volume after 2 times of 95% above alcohol of food grade stirs and leaves standstill 30 minutes;
f, drying
the distilled water or other stirring solvent that step e alcohol hypostasis are added in mass ratio 3 times make it dissolve, then, at vacuum tightness 0.01 ~ 0.090MPa, under temperature 60 C condition after vacuum-drying, yield can be obtained and reach 9.006%, 8.829%, 8.985%, sugar degree reaches 12.87%, the polysaccharide product of 13.45%, 13.64%.
the raw material that fungus polysaccharide is prepared in described extraction is that mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers., glossy ganoderma, black fungus, Grifola frondosa, white fungus, needle mushroom etc. are containing any one or a few the combination in the pharmaceutical fungi and edible fungi of compound of polysaccharide.
described extraction agent refers to that water, ethanol, acetone, ether, alkali, acid, salt etc. are for extracting the material preparing fungus polysaccharide.
in described B (2) step multistage solvent circulation Dynamic Thermal refluxing extraction be as required 1 ~ 3 grade any adjustable, both 1 grade of solvent circulation Dynamic Thermal backflow can be carried out separately when extracting, 2 grades of solvent circulation Dynamic Thermal backflows can be carried out again when single-action concentrates, also can carry out 3 grades of solvent circulation Dynamic Thermal backflows when economic benefits and social benefits concentrate.
the step of described (3) filter with concentrated in filtration be adopt order number to be that 60 ~ 200 object secondary Stainless Steel Wire net filtrations or tubular type or link-suspended basket centrifuge filter.
in described (5) drying step, vacuum freezedrying is at vacuum tightness 25 ~ l00Pa, vacuum freezedrying under temperature 20 ~ 40 DEG C of conditions; Or vacuum-drying is at vacuum tightness 0.01 ~ 0.085MPa, the vacuum-drying under temperature 45 ~ 75 DEG C of conditions.
beneficial effect of the present invention: a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method of the present invention, extracting cycle shortens, solvent load is few, production efficiency is high, energy-saving and cost-reducing, the extracting method that the wide aperture ion exchange resin of the edible and medicinal fungi polysaccharide that DNA purity is higher and a kind of low-temperature atmosphere-pressure plasma extraction process combine.Here it should be noted that low-temperature atmosphere-pressure plasma treatment process is only applied to material surface modifying process, while guarantee can not change fungus polysaccharide structure and effect, can extract efficiently and prepare the high edible and medicinal fungi polysaccharide of purity.
Embodiment
in order to make object of the present invention, technical scheme and advantage clearly understand, below in conjunction with embodiment, the present invention is further elaborated.Should be appreciated that the specific embodiment of description described herein is only in order to explain the present invention, is not intended to limit the present invention.All material rates are counted all in mass ratio in these embodiments.
embodiment 1
a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extraction process, is characterized in that: comprise following processing step:
a, polymeric adsorbent pre-treatment
after being soaked with deionized water by the S5428 resin of 1.6cm × 100cm, dress post, uses deionized water balance resin, until the liquid flowed out is not muddy;
b, fungus polysaccharide tentatively extract
(1) raw material pulverizing mixes with extraction agent
by extracting, the raw material preparing fungus polysaccharide is cleaned, cryodrying, is ground into the particle of 100 ~ 10000um, by itself and extraction agent in mass ratio 1:4 ~ 1:10 carry out Homogeneous phase mixing;
(2) extract
above-mentioned raw materials and extraction agent mixed solution are carried out circumfluence distillation, Extracting temperature 65 ~ 110 DEG C, pH=6 ~ 9, refluxing extraction 70 ~ 120 minutes under the condition of solvent refluxing rate 10 ~ 25% in multifunctional multistage solvent circulation Dynamic Thermal refluxing extraction device;
(3) filter with concentrated
by vacuum handling direct after the centrifuging of said extracted liquid in external circulation heating formula economic benefits and social benefits vacuum concentrator, at vacuum tightness 0.03 ~ 0.08MPa, concentrate 2 ~ 4 hours under temperature 50 ~ 95 DEG C of conditions, make the density of concentrated solution reach 1.2 ~ 1.50g/cm
3
;
(4) alcohol precipitations
above-mentioned concentrated solution is pumped into Alcohol-settling tank, and add by volume after 4 ~ 6 times of 97% alcohol stirs and leave standstill 90 ~ 180 minutes, obtain alcohol precipitation extract, alcohol used is more than food grade;
c, low-temperature atmosphere-pressure plasma extract
the alcohol precipitation extract that step B (4) obtains is put into low-temperature atmosphere-pressure plasma treatment appts, processes with following processing parameter: discharge frequency is 5 ~ 30KHz; Extraction time is 5 ~ 13s; Discharge gas is ammonia, and flow velocity is 0.5 ~ 5ml/min, obtains edible and medicinal fungi polysaccharide crude;
d, macroporous adsorbent resin extract
the edible and medicinal fungi polysaccharide crude obtained by step C adds water, the macroporous adsorptive resins in wet method in steps A, successively with concentration be 0.5,1.0,2.0, the NaCl solution of 3.0mol/L and 4.0mol/L carries out wash-out, elution speed is 2.0 ~ 10.0ml/min.By elutriant concentrating under reduced pressure, obtain edible and medicinal fungi polysaccharide macroporous adsorbent resin extract;
e, secondary alcohol precipitation
the fungus polysaccharide macroporous adsorbent resin extract obtained by step D pumps into Alcohol-settling tank, adds more than 5 times of 97% food grade by volume.100 minutes are left standstill after alcohol stirs;
f, drying
the distilled water or other stirring solvent that step e alcohol hypostasis are added in mass ratio 3 times make it dissolve, then, at vacuum tightness 0.03 ~ 0.09MPa, under temperature 60 C condition after vacuum-drying, yield can be obtained and reach 9.112%, 9.098'%, 8.956%, sugar degree reaches 12.96%, the polysaccharide product of 13.25%, 13.44%.
embodiment 2
identical with the step of EXAMPLE l, difference is:
b, fungus polysaccharide tentatively extract
(1) by extracting after the raw material (lotus flower bacterium, mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers.) preparing fungus polysaccharide is placed in 50 DEG C of dryings, be ground into the particle of 1500-2500um, by its with extraction agent water in mass ratio 1:6 mix;
(2) extraction conditions is: Extracting temperature 90 DEG C, refluxes and (adopt under the condition of pH=5.5. solvent refluxing rate 15%
with 3 grades of solvent circulation Dynamic Thermal backflows) extract 90 minutes;
(3) concentrated: at vacuum tightness 0.02MPa, concentrate 4 hours under temperature 60 C condition;
(4) alcohol precipitations: add by volume after 2 times of 97% above alcohol of food grade stirs and leave standstill 120 minutes;
c, low-temperature atmosphere-pressure plasma extract
the alcohol precipitation extract that step B (4) obtains is put into low-temperature atmosphere-pressure plasma treatment appts, processes with following processing parameter: discharge frequency is 10 ~ 25KHz; Extraction time is 8 ~ 15s; Discharge gas is ammonia, and flow velocity is 1.5 ~ 3.0ml/min, obtains edible and medicinal fungi polysaccharide crude;
d, macroporous adsorbent resin extract
the edible and medicinal fungi polysaccharide crude obtained by step C adds water, the macroporous adsorptive resins in wet method in steps A, successively with concentration be 0.5,1.5,3.0, the NaCl solution of 4.5mol/L and 6.0mol/L carries out wash-out, the speed of wash-out is 4.0 ~ 8.0ml/min.By elutriant concentrating under reduced pressure, obtain edible and medicinal fungi polysaccharide macroporous adsorbent resin extract;
e, secondary alcohol precipitation
the fungus polysaccharide macroporous adsorbent resin extract obtained by step D pumps into Alcohol-settling tank, adds more than 3 times of 97% food grade by volume.120 minutes are left standstill after alcohol stirs;
f is dry
the distilled water or other stirring solvent that step e alcohol hypostasis are added in mass ratio 3 times make it dissolve, then, at vacuum tightness 0.01 ~ 0.09MPa, under temperature 60 C condition after vacuum-drying, yield can be obtained and reach 19.21%, 19.98%, 18.46%, sugar degree reaches 22.59%, the polysaccharide product of 23.15%, 24.85%.
embodiment 3
identical with the step of embodiment 1, difference is:
b, fungus polysaccharide tentatively extract
(1) by extracting after the raw material (lotus flower bacterium, mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers.) preparing fungus polysaccharide is placed in 60 DEG C of dryings, be ground into the particle of 5000 ~ 8000um, by its with extraction agent water in mass ratio 1:13 mix;
(2) extraction conditions is: Extracting temperature 90 DEG C, pH=9.0, and under the condition of solvent refluxing rate 30%, backflow (is adopted
with 2 grades of solvent circulation Dynamic Thermal backflows) extract 100 minutes;
(3) concentrated: at vacuum tightness 0.05MPa, concentrate 3 hours under temperature 90 DEG C of conditions;
(4) alcohol precipitation: add by volume after 5 times of 97% above alcohol of food grade stirs and leave standstill 150 minutes;
c, low-temperature atmosphere-pressure plasma extract
the alcohol precipitation extract that step B (4) obtains is put into low-temperature atmosphere-pressure plasma treatment appts, processes with following processing parameter, obtain edible and medicinal fungi polysaccharide crude: discharge frequency is 15 ~ 30KHz; Extraction time is 10 ~ 15s; Discharge gas is ammonia, and flow velocity is 1.8 ~ 3.5ml/min;
d, macroporous adsorbent resin extract
the edible and medicinal fungi polysaccharide crude obtained by step C adds water, the macroporous adsorptive resins in wet method in steps A, successively with concentration be 1.0,2.0,4.0, the NaCl solution of 6.0mol/L and 8.0mol/L carries out wash-out, the speed of wash-out is 4.0 ~ 8.0ml/min.By elutriant concentrating under reduced pressure, obtain edible and medicinal fungi polysaccharide macroporous adsorbent resin extract;
e, secondary alcohol precipitation
the fungus polysaccharide macroporous adsorbent resin extract obtained by step D pumps into Alcohol-settling tank, adds more than 5 times of 97% food grade by volume.150 minutes are left standstill after alcohol stirs;
f is dry
the distilled water or other stirring solvent that step e alcohol hypostasis are added in mass ratio 3 times make it dissolve, then, at vacuum tightness 0.01 ~ 0.09MPa, under temperature 60 C condition after vacuum-drying, yield can be obtained and reach 19.53%, 20.68.%, 18.72%, sugar degree reaches 23.43%, the polysaccharide product of 24.96%, 22.56%.
this prepares the method for fungus polysaccharide, i.e. multistage solvent circulation Dynamic Thermal refluxing extraction method of enrichment, is to integrate extraction, concentrated and solvent recuperation etc., and whole process is carried out in a closed system, can not produce the bad phenomenon such as run, drip, leak; Be aided with low-temperature atmosphere-pressure plasma to extract and macroporous adsorbent resin roughing out, reach the effect of the higher edible and medicinal fungi polysaccharide of high efficiency extraction purity, solving prior art can not the problem of high efficiency extraction high purity edible and medicinal fungi polysaccharide.
the foregoing is only preferred embodiment of the present invention, is only illustrative for the purpose of the present invention, and nonrestrictive.The all any amendments done within the spirit and principles in the present invention of those skilled in the art, equivalent replacement and improvement etc., all should be included in protection scope of the present invention.
Claims (6)
1. an edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method, is characterized in that: comprise following processing step:
A, polymeric adsorbent pre-treatment:
After being soaked with deionized water by the S5428 resin anion(R.A) of 1.6cm × 100cm, dress post, uses deionized water balance resin, until the liquid flowed out is not muddy;
B, fungus polysaccharide tentatively extract:
(1) raw material pulverizing mixes with extraction agent
Clean extracting the raw material preparing fungus polysaccharide, after cryodrying, be ground into the particle of 70 ~ 6000um, by its with extraction agent in mass ratio 1:3 ~ 1:10 mix;
(2) extract
Above-mentioned raw materials and extraction agent mixed solution are carried out circumfluence distillation, Extracting temperature 45 ~ 100 DEG C, pH=5 ~ 8 in multifunctional multistage solvent circulation Dynamic Thermal refluxing extraction device, and under the condition of solvent refluxing rate 10 ~ 25%, refluxing extraction 50 ~ 100 minutes, obtains extracting solution;
(3) filter with concentrated
After the extracting solution of said extracted certain hour being passed through secondary wire gauzee filter or centrifuging, direct vacuum handling is in external circulation heating formula economic benefits and social benefits vacuum concentrator, at vacuum tightness 0.02-0.09MPa, concentrate 2 ~ 4 hours under temperature 40 ~ 90 DEG C of conditions, make the density of concentrated solution reach 1.1 ~ 1.40g/cm3;
(4) alcohol precipitation
Above-mentioned concentrated solution is pumped into Alcohol-settling tank, and add by volume after 3 ~ 5 times of 97% alcohol stirs and leave standstill 50 ~ 150 minutes, obtain alcohol precipitation extract, alcohol used is more than food grade;
C, low-temperature atmosphere-pressure plasma extract
The alcohol precipitation extract that step B (4) obtains is put into low-temperature atmosphere-pressure plasma treatment appts, processes with following processing parameter, obtain edible and medicinal fungi polysaccharide crude: discharge frequency is 5 ~ 30KHz; Extraction time is 5 ~ 13s; Discharge gas is ammonia, and flow velocity is 0.5 ~ 5ml/min;
D, macroporous adsorbent resin extract
The edible and medicinal fungi polysaccharide crude obtained by step C adds water, macroporous adsorptive resins in wet method in steps A, successively with concentration be 0.5,1.0,2.0, the NaCl solution of 3.0mol/L and 4.0mol/L carries out wash-out, the speed of wash-out is 2.0 ~ 10.0ml/min; By elutriant concentrating under reduced pressure, obtain edible and medicinal fungi polysaccharide macroporous adsorbent resin extract;
E, alcohol precipitation
The fungus polysaccharide macroporous adsorbent resin extract obtained by step D pumps into Alcohol-settling tank, adds by volume after 2 times of 95% above alcohol of food grade stirs and leaves standstill 30 minutes;
F, drying
The distilled water or other stirring solvent that step e alcohol hypostasis are added in mass ratio 3 times make it dissolve, then, at vacuum tightness 0.01 ~ 0.090MPa, under temperature 60 C condition after vacuum-drying, yield can be obtained and reach 9.006%, 8.829%, 8.985%, sugar degree reaches 12.87%, the polysaccharide product of 13.45%, 13.64%.
2. a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method according to claim 1, is characterized in that: the raw material that fungus polysaccharide is prepared in described extraction is that mushroom, Hericium erinaceus (Bull. Ex Fr.) Pers., glossy ganoderma, black fungus, Grifola frondosa, white fungus, needle mushroom etc. are containing any one or a few the combination in the pharmaceutical fungi and edible fungi of compound of polysaccharide.
3. a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method according to claim 1, is characterized in that: described extraction agent refers to that water, ethanol, acetone, ether, alkali, acid, salt etc. are for extracting the material preparing fungus polysaccharide.
4. a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method according to claim 1, it is characterized in that: in described B (2) step multistage solvent circulation Dynamic Thermal refluxing extraction for as required 1 ~ 3 grade any adjustable, both 1 grade of solvent circulation Dynamic Thermal backflow can be carried out separately when extracting, 2 grades of solvent circulation Dynamic Thermal backflows can be carried out again when single-action concentrates, also can carry out 3 grades of solvent circulation Dynamic Thermal backflows when economic benefits and social benefits concentrate.
5. a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method according to claim 1, is characterized in that: the step of described (3) filter with concentrated in filtration be adopt order number to be that 60 ~ 200 object secondary Stainless Steel Wire net filtrations or tubular type or link-suspended basket centrifuge filter.
6. a kind of edible and medicinal fungi polysaccharide low-temperature atmosphere-pressure plasma extracting method according to claim 1, it is characterized in that: in described (5) drying step, vacuum freezedrying is at vacuum tightness 25 ~ l00Pa, vacuum freezedrying under temperature 20 ~ 40 DEG C of conditions; Or vacuum-drying is at vacuum tightness 0.01 ~ 0.085MPa, the vacuum-drying under temperature 45 ~ 75 DEG C of conditions.
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| CN105754002A (en) * | 2016-04-29 | 2016-07-13 | 江苏耐雀生物工程技术有限公司 | Preparation method of high-content tremella polysaccharide |
| CN105902433A (en) * | 2016-05-21 | 2016-08-31 | 广州丹奇日用化工厂有限公司 | Method for extracting agaric extract from agaric and application thereof |
| CN106589156A (en) * | 2016-12-15 | 2017-04-26 | 昆明旭日丰华农业科技有限公司 | Agaric polysaccharide extraction method |
| CN108219020A (en) * | 2016-12-13 | 2018-06-29 | 河南后羿实业集团有限公司 | A kind of extracting method of pachymaran |
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| CN108219020A (en) * | 2016-12-13 | 2018-06-29 | 河南后羿实业集团有限公司 | A kind of extracting method of pachymaran |
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